Process of manufacturing chemical compounds.



. i.; th. -tvzo s 4ivo mentioned oxorop so l,

Ummm STTES QEEGE..

Spel'cationof Lettera Patent.

rlsntemarm. 2o, tooo.

Appllotion lad June 5, 190, 8.62191 Np, 330,218#

flloofwmit moy-conm' Bq itlkgowjn that L, COURTLANDF: CM1 nl Jp., s mtiaein.- of the United States, re,- si s A y ,ra,in tghe county of Chemuxig. onwtotofi NewYorlo hwoiwontod-onow d, usefpl. Improvement in Processes apufanturin i Chomloal Compounds, of which, thet fo owing io. o, Spooioation- 'Ehior mvaontionrelatosi to: an. improvedy pgfogoss fion` thopnoductlon o compounds Ofi thoillsh and alkali o. earth; memloi whwh require, tho, useV of t o. groo` metal in theip. pro wotionl 811111.11151,- object ist@ oooomplioh sup roduction inlamalrvmer. more economiofl; to been, llitllsrto.4 attlined 1420;; ofsm os, to @sont o Ero, o lpg' pmssmgsoo p c osolromlonl bo olovilof todo@ tho. rolotivs oonsumnoios oi sodium as a metalli.. the market. 'oo ofy Sodium polis o dl will bo. nelfmb'voly igllluoodv. Simollm. thorofs] t o pofgsxb itx o?. ooolomy in tho P120#- dution. o Sodium. oymmd oo of tho Prooessn now in toohniol uso isbssed. on, tho followhg motions:

From this it will be soon that all theY sodium which, rooovered as sodium cyanid enters bho' `rooms not metallic sodium.

` mou t of metallic sodium coisuxuo .99: Play? fused, bath containing modos? '1o. s Y. Salto wllio will be deoompoood by 1 n um, ogsodlum alloy, in such a` manner;

tho combined Sodium of the bath'.

afyailable asta sopmeof sodium for. th?, end product; andaddingodium, o ,rsqdiuml ollonto ohlsfused both'. lhgonerlmylgf olplomsy bel modo olsrorfby'v opplpstloo lo the two casesalroofdy oitcdl D 1li-Bodmin booddod oo) o. mlxod. fiolooq of: Sodom hydroxil (N oQHQ and Sodium o1# trote (NNOJ ,1s the; properproporooos. namely, apppoxlmately two tsy by W'xght: oi the.1 latten. to three Rptsf tho, rm rl,s there are numerous; posohlo roootlion, s; final stateof which moyfbo ospsoosoibyrtlioz following moot/ions;

Beoctioosf I and EL tok@ plooo. oi.

Y some1 time, the. pnopondotsnpo. ot, either tion doPemling-uPootho-ooodtioo ot bolos:-

orotion ondthsllw omos@ tiooo f tulamount ol sod-iumperogii produced; Sill,

thorefore. lie betsroon tho, :osu to; olllo tion,-

Llsleaotion EI, and neoctlon' lL o. #mi

tagrm of; Na. osoproduood, bx lhs oss, jot. LSfl grams o fmemllo No, on 1i groom. o? fNo-.Ol Hommes tho uso.- off 0,39 @ook No. lu momen. 111;, 23A growl o Q1 amplio; dom byfussoffooswmotmto llo- Soshwo or l; gro; Noli). momes 0:1196 mom. @on Y tallo sodlpm- L all. *llamo-oi tho; oboyom: otions woll who? f f b Prooodo ook 'ried out on a commercio scale, tho ount ofl sodium roquired por gram ol; No,V produced will vary between. the; limjts 0.393 :ind

0.196, or. a., saving in sodiuxgxg` consumption o from 33,4% to 66.7%. This slameofx'xinciplo may be. aplied to the production sodimm cyanid; metallic sodium be added 19,9,

fused bath ot NaOH in which carbon isn s ugsfy ponded and NH3 gos bo buhbled throu h, melted mass at the same tuyo, thifollwmg reaction takes placa-z this way only 2.3 mstsllc No. aro roqois'ed, to. psoduoo. 9% of: NsQN-,

`whereas by previous known methods, it

-able melte .advantage to be gained 1f sodium can be apwould require 46 grams of metallic Na, thus saving 50% in the consumption of metallic sodium. c

Sodium peroxid and sodium cyanld may be made as outlined above by the addition of previously repared metallic sodium to suitd] baths, but there is still further plied in a form, or under conditions, more economical than previously prepared metallic sodium. It is obvious that, in the above outlined process, or in that' about to be described, the substances available for the fused baths need not necessarily be confined to those which produce only the product desired and gaseous products, Vfor the formation of solid by-products will not interfere with the process if such solidgiroducts can be readil se arated from the iinished product. It as een sugoested frequently that in the manufacture of this lclass of sodium products, sodium alloys might be used in place of sodium. This, however, seems not to have been done in practice, either because such alloys are not strong enough in their action, or because no practical method has hitherto been devised for making use of vthis vague suggestion. The sim le addition of lead-sodium alloy in place o sodium to such a bath as was speci'ried above for making oxids of sodium is not fpracticable because lead would be oxidize as well as sodiumand the sodium oxid would be contaminated with sodium plumbate. Like- Wise the alloy could not be used in the formation of sodium cyanid because the alloy produced in practice has not sufficient rec ucing power to give the desired result. To make practicable the use of a lead-sodium alloy, it 1s necessary to devise a continuous` process under such conditions that the reaction with the Na can be obtained without interference of the lead. The following description is a specific application of this principle which will enable one skilled in the art to obtain oxids of sodium by such a method.

In carryinvp out my improved, process lead-sodium atlloy is first produced by any of the well known methods. Ihis is most practically done by electrolyzin a molten bath of sodium chlorid (NaCl) Wii a graphite anode and a molten lead cathode. lhe leadsodium alloy is caused to circulate by any convenient mechanical means, an is conveyed to and from a second compartment adjoining the one in which the decom osition of the sodium chlorid was affecte 'Ihe lead-sodium alloy in this second compartment is covered to a convenient depth with a fused hath of sodium hydrexid. 'l his bath of NaOH is then electrolyzed using iron,

nickel or other suitable metal for the cathode and the lead-sodium alloy as a soluble anode. Upon passing the current,'N a would be dissolved from the sodium-lead anode and ydeposited at the cathode. 1f, however, NaNO 1s added, at intervals in amount roportional to the number of amperes used t e sodium of the lead-sodium alloy will be consumed as fast as liberated according to the following reaction:

The relative values of the factors a, b, c and an, y, z will depend upon the condition of the operation as previously explained. 'Ihis mixture of N a,O -l- Na, can loe` entirely converted into Na20, by solidifying, pulverizing and heatin the powder to over 300 C. in air free from C, and H,O. 'Ihe lead-sodium alloy which has been partly depleted of its sodium is continuously returned to the first compartment, by means of the circulatin device, where it again acts as cathode and takes up more sodium to be in turn removed in the second compartment. he roduction of cyanid of sodium is conducts in the same way, except that a different electrolyte must be used 1n the second compartment. In this case the fused NaOH holds carbon in suspension. rlhe bath is electrolyzed as before and ammonia as is bubbledthrough the electrolyte, in p ace of the NaNO, used when sodium oxid wasdesired. From these two concrete examples, it will be seen that the successful use of lead-sodium alloy, as a substitute for pure sodium, rests on the use of that alloy as a soluble anode in the electrolysis of a fused bath, which is consumed in the process, thus economizing in the theoretical quantity of metallic sodium consumed and yielding only the desired product* or by-products that are readily separated therefrom. It is .also obvious, to one skilled in the art, that other com ounds than those of sodium can be prepared) in a similar manner, lthe only requisite being that such metal will alloy with a less positive metal such alloy being capable of acting as a soluble anode 1n a manner substantially as described. r[he inert metal is also not limited to lead. It is also evident that this process does not a pl to any salts of the above class of metals wlilc depend u on the action of water for their formation, or the Iabove reactions take place only in the dry, or fused state; The scope of the invention is also limited by the small number of possible electrolytes that melt within practicable limits.

An ap aratus designed for carrying out the above ascribed recess on a commercial basis, is describe by me in a co-pending application, led June 9, .1906, Serial No, 32%,98'L '1r he vaine of this process ies in the production of more of the final product than could be produced from the actual quantity of the metal entering into the reaction as metal or alloy only. That is, I makeuthe metal contained in the fused salt of the second compartment available as a substitute for a ortion of the metal which would otherwise ave to be supplied in full quantity.

What I claim as my invention and desire to secure by Letters-Patent is:

1. rlhe process of roducing compounds of the alkali and alka 'ne earth metals which consists in subjecting a fused bath containing a salt of said metal which will react With the metal to form the desired product to electrolysis with a soluble anode com risi a fused alloy of the metal with a meta Whic is electro-negative thereto. l

2. 'Ihe process of roducing compounds of the alkali and alka ine earth metals which consists in continuously producing a fused alloy, of which said metal is the more electroppsitive constituent, by the electrolysis of a sed bath containing said metal with a fluid cathode comprising a metal which is electrone ative to said metal, and continuously uti 'zing the said more electro-positive constituent of said alloy in electrolysis with a fused bath containing a salt of said metal which will react with the metal to form the desired product.

3. 'l he process of producing compounds of the alkali and alkaline earth metals, which consist in subjecting a fused soluble anode which contains the metal to electrolysis with a fused bath containin a salt of said metal which will react with t e metal to form the desired product, said bath being consumed in producing the compound.

4. 'lhe process of manufacturing sodium oxids, which consists in adding metallic sodium to a bath consisting of melted N aNOl and NaOH, in the roortions of approximatell7 two parts of a C)3 to three parts of NaO substantially as herein set forth.

5. The process o manufacturing sodium oxids, which consists in continuously roducin an alloy of sodium by the electro is of a sed bath containing sodium Wit a fluid cathode comprising a metal `which is electro-negative to sodium, and using the alloy so produced as a fused soluble anode in a bath containing a melted salt of sodium Which will re-act with the sodium of the alloy to form the desired oxid.

6. rlhe process of manufacturing sodium oxids, which consists in continuously roducin an alloy of sodium by the electro ysis of a ed bath containing sodium with a fluid cathode comprising a metal which is electro-negative to sodium, and utilizing the alloy so produced as a fused soluble anode in a bath composed of melted NaOH and N aNO to which more NaOH and NaNOa are added from time to time, as the bath is consumed.

7. 'lhe process of manufacturing sodium peroxid, which consists in the continuous production of sodium oxids by the electrolysis, with a fused soluble anode containin sodium, of a bath containing melted sa ts of sodium which will react with metallic sodium to produce sodium oxids, and heatin the oxids so produced to over 300 C. in uri ed air or oxygen.

n testimony whereof I have aliixed my signature, in presence of two witnesses.

COURTLAND F. CARRIER, JR. Witnesses:

J. H. OBamN, A. S. Divan. 

